CN103140279A - Micromixer - Google Patents

Micromixer Download PDF

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Publication number
CN103140279A
CN103140279A CN2011800474568A CN201180047456A CN103140279A CN 103140279 A CN103140279 A CN 103140279A CN 2011800474568 A CN2011800474568 A CN 2011800474568A CN 201180047456 A CN201180047456 A CN 201180047456A CN 103140279 A CN103140279 A CN 103140279A
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CN
China
Prior art keywords
fluid
stream
plate
small tubulose
tubulose stream
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Pending
Application number
CN2011800474568A
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Chinese (zh)
Inventor
石山文彦
飞泽猛
中村正幸
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DIC Corp
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Dainippon Ink and Chemicals Co Ltd
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Publication date
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Publication of CN103140279A publication Critical patent/CN103140279A/en
Pending legal-status Critical Current

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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D9/00Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • F28D9/0031Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits for one heat-exchange medium being formed by paired plates touching each other
    • F28D9/0037Heat-exchange apparatus having stationary plate-like or laminated conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall the conduits for one heat-exchange medium being formed by paired plates touching each other the conduits for the other heat-exchange medium also being formed by paired plates touching each other
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40Static mixers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/30Micromixers
    • B01F33/301Micromixers using specific means for arranging the streams to be mixed, e.g. channel geometries or dispositions
    • B01F33/3012Interdigital streams, e.g. lamellae
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90Heating or cooling systems
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F35/00Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
    • B01F35/90Heating or cooling systems
    • B01F35/92Heating or cooling systems for heating the outside of the receptacle, e.g. heated jackets or burners
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093Microreactors, e.g. miniaturised or microfabricated reactors
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C269/00Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
    • C07C269/02Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups from isocyanates with formation of carbamate groups
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/67Unsaturated compounds having active hydrogen
    • C08G18/671Unsaturated compounds having only one group containing active hydrogen
    • C08G18/672Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28FDETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F3/00Plate-like or laminated elements; Assemblies of plate-like or laminated elements
    • F28F3/08Elements constructed for building-up into stacks, e.g. capable of being taken apart for cleaning
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00783Laminate assemblies, i.e. the reactor comprising a stack of plates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00819Materials of construction
    • B01J2219/00822Metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00851Additional features
    • B01J2219/00858Aspects relating to the size of the reactor
    • B01J2219/0086Dimensions of the flow channels
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00873Heat exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781Aspects relating to microreactors
    • B01J2219/00889Mixing

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • General Engineering & Computer Science (AREA)
  • Dispersion Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Accessories For Mixers (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A micromixer comprising: a stack portion in which a first plate having a first microtubular flow path leading to a fluid supply path through which a first fluid flows, and a second plate having a second microtubular flow path through which a second fluid flows and which leads to a fluid supply path through which the second fluid flows are stacked; and a mixing portion which leads to the outlet of the first microtubular flow path and the outlet of the second microtubular flow path and in which the first fluid and the second fluid are mixed, wherein the first plate and/or the second plate comprises an inlet portion of the microtubular flow path leading to the fluid flow path and an outlet portion of the microtubular flow path leading to the mixing portion, the microtubular flow path in the inlet portion is one flow path, and the cross-sectional area of the fluid liquid-tightly flowing through the microtubular flow path in the outlet portion is smaller than the cross-sectional area of the fluid liquid-tightly flowing through the one microtubular flow path in the inlet portion.

Description

Micro-mixer
Technical field
Even the present invention relates to a kind of in the situation that mix high viscosity fluid each other, mix the fluid that low viscosity fluid and viscosity exceed 3000 times of left and right of this fluid, also can avoid the low viscosity fluid intermittent entry and the micro-mixer that mixes with the state of stablizing liquor charging.
Background technology
In the particulate manufacturing process that has utilized crystallization etc. to carry out, chemical reaction process, propose to have to mix the various static mixers that two or more at least fluids is purpose.Wherein, the micro-mixer of supplying with the fluid that mixes in the miniature stream is attracted attention by the people as a kind of efficient mixing arrangement.
Micro-mixer has following mechanism: it is that the miniature stream of 10 μ m to 1000 μ m left and right will two or more at least fluids be divided into small liquid and flows that this mechanism is used for utilizing flow path width, and after mix.Owing to being divided into small liquid stream and causing diffusion length to shorten by being supplied to fluid in micro-mixer, mixing velocity is accelerated, and therefore compares with static mixer in the past, can mix efficiently at short notice.
As the structure of micro-mixer, the known blender (Y shape micro-mixer) that the structure of the stream that for example has Y-shaped is arranged.The Y-shaped micro-mixer has following structure: the stream that flows for first fluid and the stream that flows for second fluid is acute angle, be that Y-shaped ground intersects on a plate, thereby form a converging roads.Each fluid that is supplied to this blender is sentenced the laminar condition interflow at the cross part of stream, and the phase counterdiffusion, and is then mixed.
At the fluid (anisotropic viscosity fluid) that makes low viscosity fluid and viscosity exceed 10 times of left and right of this fluid with identical flow in the situation that circulate in above-mentioned Y-shaped micro-mixer, want to make the crushing of two kinds of fluids identical.That is, accelerate the flow velocity of the lower fluid of viscosity, dwindle the use cross section ratio of miniature stream.The flow velocity of the fluid that the viscosity that slows down on the contrary is higher also increases the use cross section ratio of miniature stream, thereby makes the crushing of two kinds of fluids form identical.In the situation that differences in viscosity is large to a certain degree, the fluid that viscosity is lower flows in minimum cross section with flow velocity at a high speed, thereby becomes the reason that causes the unsettled liquid streams such as intermittent entry.Therefore, have that fluid can't stably circulate, the problem of fluid-mixing equably.
In addition, even in the situation that increase accordingly the flow path cross sectional area of the miniature stream of interflow section with the differences in viscosity of two kinds of fluids, also can increase the mutual diffusion time of liquid, and the Combination of fluid also can descend.Like this, in miniature stream during the phase counterdiffusion, mix low viscous fluid existing problems scarcely each other, but when mixing anisotropic viscosity fluid, high viscosity fluid, the possibility of the problem that multiple Combination descends is higher at liquid.
As other micro-mixers except above-mentioned Y-shaped micro-mixer, known have a cascade type micro-mixer that for example has following structure: this structure is by the plate and folded form (for example, with reference to the patent documentation 1) of the flaggy that is formed with the micro-channel that flows for reactant B of the micro-channel that will be formed with the reactant A that is provided as blending objects and flow.Each micro-channel that this cascade type micro-mixer has is the state configuration of acute angle when observing with the upper surface of slave plate, each fluid collaborates in the chamber, interflow of the outlet that is arranged at each micro-channel, and then mixed.
The micro-mixer that the described chamber, interflow that is provided with stacked structure and fluid is collaborated of patent documentation 1 forms (outlet mixed type micro-mixer) has following structure: form miniature stream on each plate of two plates that stacked on top of one another configures, formed each miniature stream is towards mixing chamber and intersection as shared outlet.In addition, the flow path width of the blender of patent documentation 1 and the degree of depth are below 250 μ m, and being easy to fluid take the instantaneous mixing of low viscosity as object, rather than with high viscosity fluid each other, blender that the anisotropic viscosity fluid-phase is corresponding.Therefore, be in the described blender of patent documentation 1 there be in the situation of high viscosity fluid, anisotropic viscosity fluid circulation, might produce crushing, obstruction etc., thereby make circulation become difficult, can't mix fully.
Patent documentation 1: the special table of day bar flat 9-512742 communique (12 pages, the 3rd figure)
Summary of the invention
Mix even the first problem of the present invention provides a kind of high viscosity fluid each other, mix the fluid that low viscosity fluid and viscosity exceed 3000 times of left and right of this fluid, also can mixing efficiency well, the micro-mixer that mixes equably, the second problem provides a kind of and uses above-mentioned micro-mixer to obtain differences in viscosity apart from the method for the mixed liquor of larger fluid, and the 3rd problem provides a kind of method of making various compounds with the method that obtains above-mentioned mixed liquor.
people of the present invention have carried out conscientious research in order to address the above problem, it found that, in having the cascade type micro-mixer of the plate that will be formed with the micro-channel that the reactant A that is provided as blending objects flows and the folded structure that forms of the flaggy that is formed with the micro-channel that flows for reactant B, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of at least one of above-mentioned plate is a stream, and, the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of the export department that is communicated with mixing section of this plate is little, even thereby in the situation that mix high viscosity fluid each other, mix in the situation of the fluid that low viscosity fluid and viscosity exceeds this fluid 3000 times of left and right, also can mixing efficiency well, can not cause the low viscosity fluid intermittent entry, the state of stablizing liquor charging mixes, by using this micro-mixer, can make rightly and use the compound of differences in viscosity apart from larger raw material, specifically, can make pigment particle with polyurethane (methyl) acrylate and anthraquinone skeleton, thereby completed the present invention.
namely, the invention provides a kind of micro-mixer, it is characterized in that, this micro-mixer has laminated section and mixing section, this laminated section forms by be laminated with the second plate on the first plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid, this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid, this mixing section is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, and mixing first fluid and second fluid, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of at least one in the first plate and the second plate is a stream, and, the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of this at least one the export department that is communicated with mixing section is little.
in addition, the invention provides a kind of manufacture method of mixed liquor, it is characterized in that, this manufacture method is used following micro-mixer, making ratio of viscosities is that 10~3000 first fluid and second fluid circulate in the first small tubulose stream and the second small tubulose stream respectively, obtain to contain the fluid-mixing of first fluid and second fluid in mixing section, above-mentioned micro-mixer has laminated section and mixing section, this laminated section forms by be laminated with the second plate on the first plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid, this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid, this mixing section is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, and mixing first fluid and second fluid, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of at least one in the first plate and the second plate is a stream, and, the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of this at least one the export department that is communicated with mixing section is little.
In addition, the invention provides the manufacture method of a kind of polyurethane (methyl) acrylate, it is characterized in that,
use the micro-mixer of following feature: this micro-mixer has laminated section and mixing section, this laminated section forms by be laminated with the second plate on the first plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid, this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid, this mixing section is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, and mixing first fluid and second fluid, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of the second plate is a stream, and, the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of the export department that is communicated with mixing section of this second plate is little,
The manufacture method of above-mentioned polyurethane (methyl) acrylate comprises:
The first operation, compound (A) with NCO is circulated in the first small tubulose stream that above-mentioned the first plate has, (methyl) acrylate (B) with hydroxyl is circulated in the second small tubulose stream that above-mentioned the second plate has, obtain to contain compound (A) and compound (B) at interior fluid-mixing in mixing section; And
The second operation makes the compound (A) in this fluid-mixing react with compound (B).
And then, the invention provides a kind of manufacture method with pigment particle of anthraquinone structure, it is characterized in that,
use the micro-mixer of following feature: this micro-mixer has laminated section and mixing section, this laminated section forms by be laminated with the second plate on the first plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid, this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid, this mixing section is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, and mixing first fluid and second fluid, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of the first plate is a stream, and, the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of the export department that is communicated with mixing section of this second plate is little,
Above-mentioned manufacture method with pigment particle of anthraquinone structure comprises:
The first operation, water (C) is circulated in the first small tubulose stream that above-mentioned the first plate has, the sulfuric acid solution (D) of the pigment with anthraquinone structure is circulated in the second small tubulose stream that above-mentioned the second plate has, at mixing section's mixing water (C) and sulfuric acid solution (D), obtain to separate out the fluid-mixing of the pigment with anthraquinone structure; And
The second operation is carried out cooling to the fluid-mixing of separating out this pigment.
Micro-mixer of the present invention is formed with small stream in the long-pending little mode of the long-pending fluid cross-section than inlet portion of the fluid cross-section of the export department of small tubulose stream.Therefore, the fluid that flows in small stream can be improved the flow velocity of fluid by pressure loss impact ground, can form turbulent flow and improves mixing efficiency.Therefore, micro-mixer of the present invention can in the situation that mix high viscosity fluid each other, mix low viscosity fluid and viscosity and mix with the state that can not cause the low viscosity fluid intermittent entry, stablize liquor charging apparently higher than the situation of the fluid of this fluid is inferior.In addition, the micro-mixer of the application of the invention, pigment particle etc. that can easily obtain polyurethane (methyl) acrylate, has an anthraquinone structure has used the compound of differences in viscosity apart from larger raw material.Particularly, adopt manufacture method of the present invention, the average grain diameter that can obtain in the past to be difficult to obtain is small pigment particle with anthraquinone structure in 10nm left and right.In the purposes of making the higher red color filter of contrast, pigment particle that this particle diameter is less is useful especially.
Description of drawings
Fig. 1 is the skeleton diagram of the micro-mixer 1 of an embodiment.
Fig. 2 is the skeleton diagram of the micro-mixer 2 of another embodiment.
Fig. 3 is the skeleton diagram of the micro-mixer 3 of another embodiment.
Fig. 4 is the exploded perspective view of the duplexer that has of micro-mixer 1.
Fig. 5 is the skeleton diagram as the first plate of the member of formation of micro-mixer 1.
Fig. 6 is the skeleton diagram as the first plate of other examples of the member of formation of micro-mixer 1.
Fig. 7 is the skeleton diagram as the first plate of other examples of the member of formation of micro-mixer 1.
Fig. 8 is the skeleton diagram as the first plate of other examples of the member of formation of micro-mixer 1.
Fig. 9 is the stereogram as the second plate of the member of formation of micro-mixer 1.
Figure 10 is the skeleton diagram as the second plate of other examples of the member of formation of micro-mixer 1.
Figure 11 is the exploded perspective view with duplexer of plate, and this plate is provided with the stream for the heat transferring medium circulation.
Figure 12 is the skeleton diagram of other routine micro-mixers.
Figure 13 is the summary construction diagram that schematically shows the device that uses in embodiment.
Figure 14 is the reaction used in embodiment with the skeleton diagram of microreactor.
The exploded perspective view of Figure 15 duplexer that to be the reaction used in embodiment have with microreactor.
Figure 16 is other the routine exploded perspective views with duplexer of plate, and this plate is provided with the stream for the heat transferring medium circulation.
Figure 17 is the summary construction diagram that schematically shows the device that uses in embodiment.
The specific embodiment
Below, according to the embodiment that Fig. 1~the present invention is specialized in Figure 17 explanation.Fig. 1 means the skeleton diagram of an example of micro-mixer 1.
Micro-mixer 1 has the housing C of hollow form, be fixed with duplexer 110 in this housing C, this duplexer 110 has be laminated with the laminated section that the second plate forms on the first plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid (F1), and this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid (F2).
Micro-mixer of the present invention is except the laminated section that stacked the first plate and the second plate form, the blender that also as exemplified in micro-mixer 1, the stacked temperature control panel that has for the heat transferring medium stream of heat transferring medium circulation forms, this gaseous mixture is stacked is: make above-mentioned the 1st stream forming portion be in position corresponding on stacked direction with above-mentioned the 1st medium stream, and make above-mentioned the 2nd stream forming portion be in position corresponding on stacked direction with above-mentioned the 2nd medium stream, the stacked heat exchange efficiency that can make is good in the above-described manner, is therefore preferred.
And, can make the equalizing temperature of fluid F 1 and fluid F 2 by stacked following temperature control panel on duplexer 110, thereby can reduce the mixing efficiency that the temperature difference because of 2 of fluid F 1 and fluid F causes reduces, therefore be preferred, above-mentioned temperature control panel has the mobile heat transferring medium stream for the thermal medium H11 of the heat exchange of carrying out 2 of fluid F 1 and fluid F.
Be provided with at the left end C1 of the housing C of above-mentioned micro-mixer 1 first fluid (F1) is supplied to first fluid supply unit 1A in housing C, be provided with at the bottom of housing C right-hand member C2 second fluid (F2) is supplied to second fluid supply unit 2A in housing C.Below, in the situation that describe in the mode of not distinguishing above-mentioned each fluid supply unit 1A, 2B, fluid supply unit 1 only is described.
Fluid supply unit 1A has the peristome 1B of the left part that is formed at housing C and is linked to the connector 1C of peristome 1B.Connector 1C is communicated with the fluid feed path that circulates for first fluid (F1), thereby this fluid feed path is communicated with the first small tubulose stream of the first plate.And, this fluid feed path is connected in interior pressurized delivered mechanism with comprising be used to the container that accumulates first fluid (F1), force (forcing) pump, the pipeline etc. that is linked to this pump, first fluid (F1) under pressurized state by this mechanism to connector 1C side pressurized delivered.At peristome 1B and be fixed between the side 11a of the duplexer 110 in housing C and be provided with the space, this space is as accumulate from the reservoir S1 performance function of the first fluid (F1) of above-mentioned pressurized delivered mechanism output temporarily.
Fluid supply unit 2A has the peristome 2B of the bottom right-hand member that is formed at housing C and is linked to the connector 2C of peristome 2B.Connector 2C is communicated with the fluid feed path that circulates for second fluid (F2), thereby this fluid feed path is communicated with the second small tubulose stream of the second plate.And, this fluid feed path is connected in interior pressurized delivered mechanism with comprising be used to the container that accumulates second fluid (F2), force (forcing) pump, the pipeline etc. that is linked to this pump, second fluid (F2) under pressurized state by this mechanism to connector 3B side pressurized delivered.At peristome 1B and be fixed between the side 11b of the duplexer 110 in housing C and be provided with the space, this space is as accumulate from the reservoir S2 performance function of the second fluid (F2) of above-mentioned pressurized delivered mechanism output temporarily.
In addition, be formed with at the bottom of housing C left end C3 thermal medium H1 is supplied to thermal medium supply unit 3A in housing C.Identical with above-mentioned fluid supply unit 1A, 2A, thermal medium supply unit 3A has peristome 3B, connector 3C.The thermal medium H1 that is supplied to thermal medium supply unit 3A is by being formed at the stream in duplexer 110, from the thermal medium efferent 4A of the upper end C4 that is formed at housing C to the outside output of housing C.Identical with above-mentioned fluid supply unit 1A, 2A, thermal medium efferent 4A has respectively peristome 4B, connector 4C.
In addition, the right-hand member C4 of housing C has efferent 5A, and this efferent 5A is made of with the connector 5C that is linked to peristome 5B the peristome 5B of the right part that is formed at housing C.At peristome 5B and be fixed between the side 11c of the duplexer 110 in housing C and be provided with the space, this space is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, the mixing S3 of the section performance function of mixing with second fluid as first fluid.As the volume of S3, the intensity of the stable circulation of the pressure loss, high viscosity fluid and anisotropic viscosity fluid that the need consideration produces, mixing force, device.The volume of S3 can be with the viscosity of each fluid, change accordingly as degree of mixing of purpose etc.Particularly, for making the different two or more fluid of viscosity (anisotropic viscosity fluid) circulation, can reaching the viewpoint of stable circulation when mixing, as the preferred 100mm of the volume of S3 3Above, be more preferably 250mm 3Above.
In addition, due in the situation that the differences in viscosity between first fluid and second fluid more greatly, for example more than 10 times, the way that increases the sectional area of the mixing S3 of section in order to carry out stable circulation can obtain the uniform mixture of first fluid and second fluid, is therefore preferred.In addition, in the situation that the differences in viscosity between first fluid and second fluid is large and the flow of the flow-rate ratio low viscosity fluid of high viscosity fluid is large, the preferred sectional area that further increases mixing section.
For the viewpoint that can obtain to have mixed well the mixture that first fluid and second fluid form, preferably the area of section that is communicated with of the above-mentioned mixing S3 of section and outlet outlet the first small tubulose stream and the second small tubulose stream is 50mm 2Above, 100mm more preferably 2Above.
In addition, the area of section that the outlet above-mentioned mixing S3 of section and outlet the first small tubulose stream and the second small tubulose stream is communicated with is the low viscosity fluid stably circulation incessantly that the micro-mixer of 5 times~50 times of summation of sectional area of the outlet of the sectional area of outlet of the first small tubulose stream and the second small tubulose stream can make the anisotropic viscosity fluid, and can reach good mixing, therefore be preferred, be more preferably the micro-mixer of 10 times~200 times, further the micro-mixer of preferred 20 times~300 times.
As mentioned above, micro-mixer of the present invention can be as one sees fit be used for mixing high viscosity fluid each other, differences in viscosity is apart from larger fluid.In micro-mixer of the present invention, the first fluid that circulates in the small tubulose stream that the first plate has, the second fluid that circulates in the small tubulose stream that the second plate has flow into to mixing section.The efferent 5A of fluid from Fig. 1 that flows into to mixing section discharges outside micro-mixer, but the speed (inflow velocity) the when rate of outflow of the fluid of this moment flows into to the section of mixing with second fluid than first fluid slowly.Therefore, the invention people consider just like lower device, the liquid stream of vortex-like, the convolution stream of this device by producing fluid in mixing section, thus can utilize this liquid stream to mix efficiently first fluid and second fluid.
For being easy to produce the viewpoint that above-mentioned liquid vortex-like, convolution stream flows, distance between the export department of the section of mixing that the export department of the export department of the preferred first small tubulose stream and the second small tubulose stream and mixture for first fluid and second fluid circulate is 2mm~100mm, is more preferably 10mm~200mm.In addition, in the present invention, the export department of mixing section refers to the peristome that the 5B by Fig. 1 of mixture represents.
First fluid (F1) is by from fluid supply unit 1A to housing C internal feed, and circulate in the first small tubulose stream that is formed at duplexer 110, second fluid (F2) is by from fluid supply unit 2A to housing C internal feed, and circulates in the second small tubulose stream that is formed at duplexer 110.Then, the second fluid (F2) of the outlet of the first fluid (F1) of the outlet of arrival the first small tubulose stream and arrival the second small tubulose stream is discharged and mixes to the mixing S3 of section that is communicated with above-mentioned export department.The fluid-mixing that obtains (F3) is outside output from efferent 5A to housing C.In addition, the position of the housing C of micro-mixer 1, each fluid supply unit 1A, 2A, efferent 5A etc. is not limited to said structure, can suitably change.
As the micro-mixer of another embodiment, also can example hybrid the micro-mixer variform, shown in Figure 22 of section.In Fig. 2, the first small tubulose stream that is connected with the side 11c of duplexer 110 and the export department of the second small tubulose stream are positioned on the face that 11c caves in from the side, and this depression is as the part performance function of mixing section.
In addition, as the micro-mixer of another embodiment, also can example micro-mixer 3 shown in Figure 3.For micro-mixer 3, also identical with micro-mixer 2, the the first small tubulose stream that is connected with the side 11c of duplexer 110 and the export department of the second small tubulose stream are positioned on the face that 11c caves in from the side, are provided with in the part that caves in the pipe arrangement that fluid-mixing is discharged outside micro-mixer.Therefore, micro-mixer 3 is different from micro-mixer 2, and only sunk part is as mixing section performance function.In this case, the export department of mixing section refer to mixture by the peristome shown in the 5B ' of Fig. 3.
Then, above-mentioned duplexer 110 is described.As shown in Figure 4, duplexer 110 has the plate group 12 that is formed with stream between OBL each cover plate P1, P2.
Plate group 12 consists of by plate 7 is stacked with two the first plates 5 and two second.In the present embodiment, be formed with the alternately laminated duplexer that forms of the first plate and the second plate.
The profile of cover plate P1, P2, the first plate 5 and the second plate 7 forms identical oblong-shaped.In addition, material for cover plate P1, P2, the first plate 5 and the second plate 7 there is no particular determination, so long as such as metal material, resin, glass, pottery etc., the processing that is used to form stream is easier to and can the material that each plate interfixes be got final product with the closed state that is difficult to produce leak of liquid etc.In addition, both can form each plate with identical material, also can form with different materials each plate.For example, also can form each plate by stainless steel, and utilize diffusion bond to be fixed with closed state.The processing method of each plate can be selected the suitable method corresponding with its material in known the whole bag of tricks such as injection moulding, solvent casting, melting replica method, cutting, etching, photoetching process, laser abrasion method.
Then, be described in detail the first plate 5 and the second plate 7.As shown in Figure 5, have rectangle and the first tabular small tubulose stream forming portion 6A on the first plate 5.
The first small tubulose stream forming portion 6A is the first small tubulose stream 6 of the central portion of the width of surperficial 6a (Y-direction in figure) with one or more thereon.The first small tubulose stream 6 forms the groove shape from the left-hand end 6b of the first small tubulose stream forming portion 6A towards right-hand end 6c, and at left-hand end 6b, right-hand end 6c and upper surface 6a opening.The opening of left-hand end 6b is the entrance 6d of the first small tubulose stream 6, and the opening of right-hand end 5c is the outlet 6e of the first small tubulose stream 6.Entrance 6d is communicated with the above-mentioned first fluid supply unit 1A that supplies with first fluid F1.
The first small tubulose stream 6 is streams of the rectangular shape in cross section on direction with circulating direction phase quadrature, and extends to right-hand end 6c from left-hand end 6b.In order to ensure the uniformity of the Temperature Distribution of fluid, the intensity of device, preferably width and the degree of depth with the first small tubulose stream 6 is made as for example scope of width 0.1mm~100mm, degree of depth 0.1mm~5mm, is more preferably the scope of width 0.1mm~20mm, degree of depth 0.1mm~2mm.That is, as the shape of large-diameter portion 16, so long as crushing (pressure loss) is not excessive, be difficult to produce stream sealing, and can promptly control the heating, cooling of stream, the stream shape that can boost productivity gets final product.Preferred crushing is below 5MPa, to be more preferably below 1MPa.
In addition, the sectional area as the fluid that is liquid-tight shape circulation in the first small tubulose stream 6 is preferably 0.01mm 2~500mm 2, be more preferably 0.01mm 2~40mm 2
In Fig. 4, dispose five the first small tubulose streams 6, but there is no particular restriction for number.In the situation that dispose many, the width of each small tubulose stream 6 and the degree of depth both can be identical, also can be different.In addition, the entrance of the first small tubulose stream 6 both can be identical with the flow path width of outlet, also can be different.Fig. 6 represents the another example of the first plate.
In addition, due in above-mentioned the first plate, use with export department that mixing section is communicated with in the inlet portion of the small tubulose stream that is communicated with the fluid feed path of the sectional area ratio of small tubulose stream in the little plate of the sectional area of small tubulose stream, can obtain mixing efficiency micro-mixer preferably, be therefore preferred.Fig. 5 represents the first plate of this embodiment.Below, according to Fig. 7, this plate is described.
In Fig. 7, the first small tubulose stream 6 is provided with the less minor diameter part 6g of the larger large-diameter portion 6f of stream diameter, stream diameter and diameter from large-diameter portion 6f to tapering 6h that minor diameter part 6g changes reposefully.
Large-diameter portion 6f is the stream of the rectangular shape in cross section on direction with circulating direction phase quadrature, and extends to the front of right-hand end 6c from left-hand end 6b.In order to ensure the uniformity of the Temperature Distribution of fluid, the intensity of device, preferably the width of large-diameter portion 6f and the degree of depth are made as for example width 0.1mm~100mm, the scope below degree of depth 5mm, be more preferably the following scope of width 0.1mm~20mm, degree of depth 2mm.That is, as the shape of large-diameter portion 16, so long as crushing is not excessive, and be difficult to produce stream sealing, can promptly control the heating, cooling of stream, the stream shape that can boost productivity gets final product.Preferred crushing is below 5MPa, to be more preferably below 1MPa.
Large-diameter portion 6f is the stream of the rectangular shape in cross section on direction with circulating direction phase quadrature, and extends to the front of right-hand end 6c from left-hand end 6b.In order to ensure the uniformity of the Temperature Distribution of fluid, the intensity of device, preferably width and the degree of depth with large-diameter portion 6f is made as for example scope of width 0.1mm~100mm, degree of depth 0.1mm~5mm, is more preferably the scope of width 0.1mm~20mm, degree of depth 0.1mm~2mm.The scope of width 0.1mm~20mm, degree of depth 0.1mm~1mm more preferably.Namely, shape as large-diameter portion 16, so long as crushing is not excessive, and be difficult to produce the stream sealing, can promptly control the heating, cooling of stream, can improve the flow velocity of fluid, can act on shearing force, can form the molecular diffusion under the state of following little turbulent flow, thereby the stream shape that can improve mixing efficiency gets final product.Preferred crushing is below 5MPa, to be more preferably below 1MPa.
In addition, the sectional area as the first small tubulose stream 6f is preferably 0.01mm 2~500mm 2, be more preferably 0.01mm 2~40mm 20.01mm more preferably 2~20mm 2
Minor diameter part 6g forms the rectangular-shaped stream in cross section, and extends towards right-hand end 6c from the front of right-hand end 6f.At least the sectional area than large-diameter portion 16 is little as long as the sectional area of minor diameter part 6g forms, and is for example the scope of width 0.1mm~20mm, degree of depth 0.1mm~5mm, is more preferably the scope of width 0.1mm~5mm, degree of depth 0.1mm~2mm.The scope of width 0.1mm~5mm, degree of depth 0.1mm~1mm more preferably.Namely, shape as minor diameter part 17, so long as crushing is not excessive, and be difficult to produce the stream sealing, can promptly control the heating, cooling of stream, can improve the flow velocity of fluid, can act on shearing force, can form the molecular diffusion under the state of following little turbulent flow, thereby the stream shape that improves mixing efficiency gets final product.
In addition, the sectional area as the first small tubulose stream 6g is preferably 0.01mm 2~100mm 2, be more preferably 0.01mm 2~10mm 20.01mm more preferably 2~5mm 2
In order to improve the shearing force that acts on fluid, preferably the speed of the fluid in when circulation is 0.5m/ more than second in the first small tubulose stream 6g, is more preferably 1.0m/ more than second.More preferably 3.0m/ more than second, is particularly preferably 5.0m/ more than second.Particularly in the situation that the full-bodied fluid of mixing is each other, flow velocity that mix the larger fluid of differences in viscosity distance is preferably 1.0m/ more than second.
The first small tubulose stream 6 is streams of the rectangular shape in cross section on direction with circulating direction phase quadrature, and extends to right-hand end 6c from left-hand end 6b.In order to ensure the uniformity of the Temperature Distribution of fluid, the intensity of device, preferably width and the degree of depth with the first small tubulose stream 6 is made as for example scope of width 0.1mm~100mm, degree of depth 0.1mm~5mm, is more preferably the scope of width 0.1mm~10mm, degree of depth 0.1mm~1mm.The scope of width 0.1mm~20mm, degree of depth 0.1mm~2mm more preferably.Further be preferably the scope of width 0.1mm~2mm, degree of depth 0.1mm~0.5mm.Namely, shape as large-diameter portion 16, so long as crushing is not excessive, and be difficult to produce the stream sealing, can promptly control the heating, cooling of stream, can improve the flow velocity of fluid, can act on shearing force, can form the molecular diffusion under the state of following little turbulent flow, thereby the stream shape that can improve mixing efficiency gets final product.Preferred crushing is below 5MPa, to be more preferably below 1MPa.
In Fig. 7, dispose three the first small tubulose streams 6, but do not have particular restriction for number.In the situation that be provided with many, the width of each small tubulose stream 6 and the degree of depth both can be identical, also can be different.In addition, the entrance of the first small tubulose stream 6 both can be identical with the flow path width of outlet, also can be different.Fig. 8 represents the another example of the first plate.
The viscosity of the fluid that preferably circulates in the first small tubulose stream is below 3000mPas, more preferably below 1000mPas.More preferably below 500mPas.Further be preferably below 100mPas.
Then, be described in detail the second plate 7.As shown in Figure 9, have rectangle and the second tabular small tubulose stream forming portion 7A on the second plate 7.
The second small tubulose stream forming portion 7A has second a small tubulose stream 8 on surperficial 7a thereon.The second small tubulose stream 8 from the lower side 7b of the second small tubulose stream forming portion 7A towards width (7c direction, Y-direction in figure) form the groove shape, and then pay extreme direction bending to the right closely at right angles once in the central authorities of Y-direction, and at lower side 7b, right-hand end 7d and upper surface 7a opening.The opening of lower side 7b is the entrance 8a of the second small tubulose stream 8, and the opening of right-hand end 7d forms the outlet 8b of the first small tubulose stream 6.Entrance 8a is communicated with the above-mentioned second fluid supply unit 2A that supplies with second fluid F1.
Micro-mixer of the present invention is characterised in that, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of at least one of the first plate and the second plate is a stream, and, this at least one be the little plate (in this manual, this plate being described as the second plate) of sectional area of the small tubulose stream in the sectional area ratio inlet portion of small tubulose stream of the export department that is communicated with mixing section.By having such structure, flow in second fluid F2 entrance 8a in inlet portion, large-diameter portion, and flow into minor diameter part 8b.The second fluid F2 that flow in minor diameter part flows into outlet 8b with the large flow velocity of flow velocity when flowing into entrance, and flows into mixing section (S3 in Fig. 1).Its result can improve the mixing velocity of first fluid F1 and second fluid F2.Particularly, in the situation that at least one in first fluid F1, second fluid F2 for the lower and fluid that be difficult to mix of mobility is high viscosity fluid, differences in viscosity is inferior apart from larger situation to each other, can bring into play effect especially.
In order to ensure the uniformity of the Temperature Distribution of fluid, the intensity of device, preferably width and the degree of depth with above-mentioned large-diameter portion is made as for example scope of width 0.1mm~100mm, degree of depth 0.1mm~5mm, is more preferably the scope of width 0.1mm~20mm, degree of depth 0.1mm~2mm.That is, as the shape of large-diameter portion, so long as crushing is not excessive, and be difficult to produce stream sealing, can promptly control the heating, cooling of stream, the stream shape that can boost productivity gets final product.Preferred crushing is below 5MPa, to be more preferably below 1MPa.
In addition, as being the liquid-tight shape ground sectional area at the fluid of large-diameter portion circulation, be preferably 0.01mm 2~500mm 2, be more preferably 0.01mm 2~40mm 2
As long as the sectional area of above-mentioned minor diameter part forms less than the sectional area of large-diameter portion at least sectional area.The width of minor diameter part and the degree of depth are the following scope of width 0.1mm~20mm, degree of depth 5mm for example, are more preferably the scope of width 0.1mm~5mm, degree of depth 0.1mm~2mm.That is, as the shape of minor diameter part, so long as crushing is not excessive, and be difficult to produce stream sealing, can promptly control the heating, cooling of stream, the stream shape that can boost productivity gets final product.Preferred crushing is below 5MPa, to be more preferably below 1MPa.
In addition, as being the liquid-tight shape ground sectional area at the fluid of minor diameter part circulation, be preferably 0.01mm 2~100mm 2, be more preferably 0.01mm 2~10mm 2
In order to improve the shearing force that acts on fluid, the speed when preferably fluid circulates in the second small tubulose stream 8b is 0.5m/ more than second, is more preferably 1.0m/ more than second.More preferably 3.0m/ more than second, is particularly preferably 5.0m/ more than second.Particularly the preferred flow velocity that mixes in situation in full-bodied fluid situation each other, that mix the larger fluid of differences in viscosity distance is that 1.0m/ is more than second.
The viscosity of the fluid that preferably circulates in the second small tubulose stream is below 3000mPas, to be more preferably below 1000mPas.More preferably below 500mPas.Further be preferably below 100mPas.
In addition, as shown in Figure 9, the export department that is communicated with mixing section of the second plate is cut by a plurality of wall parts that the direct of travel with fluid arranges abreast, thereby is formed with many streams, in addition, also can be for example as shown in figure 10 example like that, form a stream.At this, the quantity of wall section is for example 1~250, is more preferably 1~50.In addition, the quantity that is formed at the second small tubulose stream on the second plate can be both shown in Figure 9 one, can be also shown in Figure 10 many.
The temperature control panel of also can be in micro-mixer of the present invention stacked medium circulation be used to heat exchange is used.For example, Figure 11 represents to be laminated with the micro-mixer that temperature control panel, the first plate and the second plate form.
As shown in figure 11, temperature control panel 12 separates the temperature adjustment stream 13 that predetermined compartment of terrain is provided with the section grooves shape on the face 12a of a side.For the sectional area of temperature adjustment stream 12, as long as can transmit heat to the reaction stream, just be not particularly limited, but be roughly 0.02(mm 2)~500.0(mm 2) scope.Be more preferably 0.05(mm 2)~40.0(mm 2).For the number of temperature adjustment stream 6, can consider heat exchange efficiency and adopt suitable number, be not particularly limited, but be for example 1~1000 on every plate, preferred 10~100.The width of preferred flow path forms for example scope of width 0.2mm~100mm, degree of depth 0.1mm~5mm, is more preferably the scope of width 0.5mm~20mm, degree of depth 0.1mm~2mm.That is, as the shape of large-diameter portion 16, so long as crushing is not excessive, and be difficult to produce stream sealing, can promptly control the heating, cooling of stream, the stream shape that can boost productivity gets final product.
As shown in figure 11, temperature adjustment stream 12 also can comprise: primary flow path 13a, and its length direction along temperature control panel 12 is arranged with many; Supply side stream 13b, its upstream side at primary flow path 13a is communicated with primary flow path 13a; And discharge effluent road 13c, its end of downstream side at primary flow path 13a is communicated with primary flow path 13a.
In Figure 11, supply side stream 13b is with to discharge effluent road 13c at right angles crooked twice, respectively from side 12d, the 12e of temperature control panel to outside opening.For the number of each stream of temperature adjustment stream 12, only the primary flow path 13a of temperature adjustment stream 12 partly is arranged with many, supply side stream 13b and discharge effluent road 13c and be made of a stream respectively.
In the duplexer 110 that consists of as described above, the first fluid (F1) of supplying with in from first fluid supply unit 1A to housing C with pressurized state after lodging in reservoir S1 temporarily, and is divided towards a plurality of first small tubulose stream 6 of being located at duplexer 110.In addition, the second fluid (F2) of supplying with in from second fluid supply unit 2A to housing C with pressurized state after lodging in reservoir S2 temporarily, and is divided towards a plurality of second small tubulose stream 8 of being located at duplexer 110.
The outlet 6e of first fluid (F1) by the first small tubulose stream 6 that flows in each first small tubulose stream 6 of the first plate 5 exports to the mixing S3 of section.In addition, the second fluids (F2) that flow in each second small tubulose stream 8 of the second plate 7 10 improve flow velocity and export to outlet 8b from large-diameter portion 9 to minor diameter part on one side, and then export to the mixing S3 of section from exporting 8b.
While improve flow velocity to the second fluid (F2) of the mixing S3 of section output with export the second fluid (F2) that mixes the S3 of section to and mix mutually.At this moment, due to the speed raising of second fluid (F2), so the mixing efficiency of the mixing S3 of section improves.
First fluid (F1) and second fluid (F2) produce turbulent flow at the mixing S3 of section on one side to be mixed on one side, and the fluid-mixing that obtains (F3) flows to the efferent 5A of fluid-mixing.Then, export outside housing C from efferent 5A.
The inlet portion of the small tubulose stream that the second plate has can be easily increased due to micro-mixer of the present invention, therefore also the fluid-mixing of multiple fluid can be obtained.In the situation that multiple fluid is circulated in micro-mixer of the present invention, the micro-mixer that can preferred exemplary for example has following laminated section: this laminated section forms by stacked at least one the first plate and two the second plates at least, and this laminated section is provided with the inlet portion of the small tubulose stream that the first plate has on the side different from the side of the inlet portion that is provided with the small tubulose stream that the second plate has.Specifically, as shown in figure 12, by stacked first plate for the circulation of E liquid and four the second plates that circulate for A liquid, B liquid, C liquid and D liquid respectively, can obtain to mix the micro-mixer of five kinds of solution.
The manufacture method of mixed liquor of the present invention is characterised in that, use micro-mixer of the present invention, making ratio of viscosities is that 10~3000 first fluid and second fluid circulate in the first small tubulose stream and the second small tubulose stream respectively, obtains to contain the fluid-mixing of first fluid and second fluid in mixing section.In the situation that used blender in the past, when mixing differences in viscosity apart from larger fluid, can produce the loss of pressure, the obstruction of fluid etc. when circulation, thereby make the circulation difficulty that becomes, can't mix fully.In manufacture method of the present invention, use micro-mixer of the present invention can not cause above-mentioned problem, even ratio of viscosities is the fluid that 10~3000 such viscosity have a long way to go, also can in the situation that not cause low viscosity fluid intermittently to form stable through-flow, can mix well.
In above-mentioned manufacture method, by supplying with to following microtubules shape stream at first fluid and the higher one of second fluid medium viscosity, can mix equably first fluid and second fluid, therefore be preferred, the inlet portion that is communicated with the fluid feed path of above-mentioned small tubulose stream is a stream, and the sectional area of the sectional area ratio inlet portion of the export department that is communicated with mixing section of above-mentioned small tubulose stream is little.The plate that in the present invention, will have such stream discloses as the second plate.
As the differences in viscosity of fluid apart from larger combination, can preferred exemplary for example combination as described below.
1. use (methyl) acrylate (A) that has the compound (A) of NCO and have hydroxyl, obtain the combination of polyurethane (methyl) acrylate.
2. use to have (methyl) acrylate of hydroxyl and the compound with epoxy radicals, obtain the combination of epoxy (methyl) acrylate.
3. use the compound with reactive hydrogen and the compound with NCO, obtain the combination of polyurethane resin.
4. use the solution that contains alkylphenol and the solution that contains hydrogen peroxide, obtain the combination of alkyl substituted benzene diphenol.
5. use sulfuric acid solution and the water of the pigment with anthraquinone structure, acquisition has the combination of pigment particle of anthraquinone structure.
Below, as the example in preferred combination, the manufacture method of polyurethane (methyl) acrylate that has used micro-mixer of the present invention is described and has the manufacture method of pigment particle of anthraquinone structure.
The manufacture method of polyurethane (methyl) acrylate
the manufacture method of polyurethane of the present invention (methyl) acrylate, it is characterized in that, use the micro-mixer of following feature: this micro-mixer has laminated section and mixing section, this laminated section forms by be laminated with the second plate on the first plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid, this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid, this mixing section is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, and mixing first fluid and second fluid, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of at least one in the first plate and the second plate is a stream, and, the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of this at least one the export department that is communicated with mixing section is little,
The manufacture method of above-mentioned polyurethane (methyl) acrylate comprises:
The first operation, make in any one in the above-mentioned first small tubulose stream or the second small tubulose stream of compound (A) with NCO and circulate, (methyl) acrylate (B) with hydroxyl is circulated in another small tubulose stream, obtain to contain compound (A) and compound (B) at interior fluid-mixing in mixing section; And
The second operation makes the compound (A) in this fluid-mixing react with compound (B).
in the manufacture method of polyurethane of the present invention (methyl) acrylate, preferably, use following micro-mixer: in micro-mixer of the present invention, the second plate has the inlet portion of the small tubulose stream that is communicated with the fluid feed path and the export department of the small tubulose stream that is communicated with mixing section, the small tubulose stream of this inlet portion is a stream, and, this second plate has be that the fluid cross-section that liquid-tight shape ground circulates is long-pending amasss little sectional area than be the fluid cross-section that liquid-tight shape ground circulates in a small tubulose stream of inlet portion in the small tubulose stream of export department,
The manufacture method of above-mentioned polyurethane (methyl) acrylate comprises:
The first operation, compound (A) with NCO is circulated in the first small tubulose stream that above-mentioned the first plate has, (methyl) acrylate (B) with hydroxyl is circulated in the second small tubulose stream that above-mentioned the second plate has, obtain to contain compound (A) and compound (B) at interior fluid-mixing in mixing section; And
The second operation makes the compound (A) in this fluid-mixing react with compound (B);
The manufacture method of above-mentioned polyurethane (methyl) acrylate is mixing cpd (A) and compound (B) well, can stable polyurethane (methyl) acrylate of quality bills of materials, and be therefore preferred.
Usually, the ratio of viscosities that has (methyl) acrylate of hydroxyl has the high 100 times of left and right of compound (A) of NCO.In the present invention, circulate in the second small stream by making the higher compound of viscosity (B), it is promptly circulated in stream, can obtain to mix equably the mixture of compound (A) with compound (B) in mixing section.
In the first operation of the present invention, obtain to contain compound (A) and compound (B) at interior fluid-mixing in the mixing section of micro-mixer.As compound (A), there are the isocyanate compounds such as fragrant family isocyanate compound, aliphatic isocyanates compound, ester ring type isocyanate compound.specifically, for example there are toluene di-isocyanate(TDI), methyl diphenylene diisocyanate, hydrogenated diphenyl methane diisocyanate, the phenylmethane polyisocyanates, modified diphenylmethane diisocyanate, XDI, hydrogenated xylene diisocyanate, hexamethylene diisocyanate, trimethyl hexamethylene diisocyanate, tetramethylxylene diisocyanate, IPDI, the ENB vulcabond, phenylene vulcabond, LDI, LTI, naphthalene diisocyanate, the 2-(methyl) acryloxy ethyl isocyanate, two (acryloyl group methyl) ethyl isocyanates of 1,1-, phenyl isocyanate, the tolysulfonyl isocyanates, octadecylisocyanate, tripolymer compound or the polymer compounds of butyl isocyanate or above-mentioned isocyanates, adduct type isocyanate compound, biuret type isocyanate compound, allophanate type isocyanate compound, uretdione (uretdione) type isocyanate compound, the reaction product of their end-blocking compound or above-mentioned isocyanates and polyalcohol.Both above-claimed cpd can be used separately, also two or more above-claimed cpds can be used.
As compound (B), for example there are (methyl) acrylic acid 2-hydroxyl ethyl ester, (methyl) acrylic acid 2-hydroxypropyl acrylate, (methyl) acrylic acid 2-hydroxy butyl ester, (methyl) acrylic acid 4-hydroxy butyl ester, 2-ethoxy acryloyl group phosphate, 2-(methyl) hydroxyl (methyl) acrylate compounds with 1 (methyl) acryloyl group of acryloxy ethyl-2-hydroxypropyl phthalic acid ester, caprolactone modification (methyl) acrylic acid 2-hydroxyl ethyl ester etc.;
2-hydroxyl-3-(methyl) hydroxyl (methyl) acrylate compounds with plural (methyl) acryloyl group of acryloxy propyl group (methyl) acrylate, pentaerythrite three (methyl) acrylate, dipentaerythritol five (methyl) acrylate, caprolactone modification dipentaerythritol five (methyl) acrylate, oxirane modification pentaerythrite three (methyl) acrylate etc. etc.Both above-claimed cpd can be used separately, also two or more above-claimed cpds can be used.
When wish obtains the fluid-mixing of compound (A) and compound (B), for example put into the container of compound (A) and the second small tubulose stream of micro-mixer as long as connect, in addition, connect container and the first small tubulose stream of putting into compound (B), use pump that each compound is circulated in small tubulose stream with flow velocity 100g/min left and right, mix getting final product in mixing section.
When compound (A), compound (B) are circulated in small tubulose stream, also can for example heat compound with 60 ℃ of left and right, viscosity is descended.
The fluid-mixing of discharging from mixing section is heated, compound (A) and compound (B) are reacted.For the temperature in when reaction, for example, when reacting with batch (-type), get final product with 70 ℃~100 ℃, in addition, when the reactors such as use pipe reactor reacted continuously, this temperature was 100 ℃~180 ℃.When using reactor to react continuously, though at high temperature react, by after reaction finishes, cooling reaction product promptly, what can prevent from reacting is out of control.
Manufacture method with pigment particle of anthraquinone structure
manufacture method with pigment particle of anthraquinone structure of the present invention, it is characterized in that, use the micro-mixer of following feature: this micro-mixer has laminated section and mixing section, this laminated section forms by be laminated with the second plate on the first plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid, this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid, this mixing section is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, and mixing first fluid and second fluid, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of at least one in the first plate and the second plate is a stream, and, the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of this at least one the export department that is communicated with mixing section is little,
Above-mentioned manufacture method with pigment particle of anthraquinone structure comprises:
The first operation, make in any one in the above-mentioned first small tubulose stream and the second small tubulose stream of water (C) and circulate, the sulfuric acid solution (D) of the pigment with anthraquinone structure is circulated in another small tubulose stream, at mixing section's mixing water (C) and sulfuric acid solution (D), obtain to separate out the fluid-mixing of the pigment with anthraquinone structure; And
The second operation is carried out cooling to the fluid-mixing of separating out this pigment.
in the manufacture method of pigment particle with anthraquinone structure of the present invention, preferably, use following micro-mixer: in micro-mixer of the present invention, the second plate has the inlet portion of the small tubulose stream that is communicated with the fluid feed path and the export department of the small tubulose stream that is communicated with mixing section, the small tubulose stream of this inlet portion is a stream, and, this second plate has be that the fluid cross-section that liquid-tight shape ground circulates is long-pending amasss little sectional area than be the fluid cross-section that liquid-tight shape ground circulates in a small tubulose stream of inlet portion in the small tubulose stream of export department,
Above-mentioned manufacture method with pigment particle of anthraquinone structure comprises:
The first operation, water (C) is circulated in the first small tubulose stream that above-mentioned the first plate has, the sulfuric acid solution (D) of the pigment with anthraquinone structure is circulated in the second small tubulose stream that above-mentioned the second plate has, at mixing section's mixing water (C) and sulfuric acid solution (D), obtain to separate out the fluid-mixing of the pigment with anthraquinone structure; And
The second operation is carried out cooling to the fluid-mixing of separating out this pigment; The manufacture method of above-mentioned pigment particle with anthraquinone structure is mixing water (C) and sulfuric acid solution (D) efficiently, can obtain less pigment particle of average grain diameter, is therefore preferred.
The high 30 times of left and right of ratio of viscosities water (C) of sulfuric acid solution (D) with pigment of anthraquinone structure.In the present invention, by the higher sulfuric acid solution of viscosity (D) is circulated in the second small stream, this sulfuric acid solution (D) is promptly circulated in stream, can obtain to have mixed equably in mixing section the mixture of compound (A) and compound (B).
The first operation of the present invention is following operation: in the first operation of the present invention, at mixing section's mixing water (C) and the sulfuric acid solution (D) of micro-mixer, obtain to separate out by crystallization the fluid-mixing of the pigment with anthraquinone structure.As having for anthraquinone (the ア Application ト ラ キ ノ Application that obtains sulfuric acid solution (D)?) pigment of structure, there are such as C.I. pigment Red 83, C.I. paratonere 177, C.I. pigment Red 89 etc.Wherein, the less pigment particle of particle diameter is sub for obtaining, and can be suitably as the viewpoint of the red filter joint (filter segment) that consists of colour filter, preferred C.I. paratonere 177.
To have the pigment dissolved of anthraquinone structure in the concentration of the sulfuric acid of the sulfuric acid solution (normal temperature viscosity 27mPas) of sulfuric acid for being used for modulation, as long as be dissolved with the pigment with anthraquinone structure, and can not be subject in the scope of the chemical reactions such as sulfonation, oxidation, just there is no particular determination, but be generally the scope of 70 % by weight~100 % by weight, as long as particularly can use the concentrated sulfuric acid of selling in the market of 95 % by weight~98 % by weight, just comparatively favourable in economy, operating aspect.
The containing ratio of the pigment with anthraquinone structure in sulfuric acid solution is required to be 2 quality %~25 quality %.If containing ratio lacks than 2 quality %, be difficult to have both the quality of pigment of the particle diameter of the efficiency of production and Nano grade, therefore not preferred.If containing ratio is more than 25 quality %, separate out again because the impact of airborne moisture etc. causes pigment to produce, thereby be difficult to obtain the pigment of the particle diameter of Nano grade, therefore not preferred.The containing ratio of the pigment with anthraquinone structure in preferably sulfuric acid solution is 3 quality %~20 quality %, is more preferably 4 quality %~15 quality %.
When making sulfuric acid solution, for chemical reactions such as the sulfonation that prevents from causing the pigment with anthraquinone structure, oxidations, the mode that preferably forms below 45 ℃ with the temperature of sulfuric acid solution is mixed pigment and the sulfuric acid with anthraquinone structure, and the mode that is more preferably to form 32 ℃~42 ℃ is mixed.
In order to obtain to separate out the fluid-mixing of the pigment with anthraquinone structure, as long as for example connect and put into the container of sulfuric acid solution (D) and the second small tubulose stream of micro-mixer, in addition, connect container and the first small tubulose stream of putting into water (C), by using pump that each fluid is circulated in small tubulose stream to each compound, and mix in mixing section and get final product.In the first operation, sub owing to mixing the water (C) of 300 Quality Mgmt Dept~3000 Quality Mgmt Dept and can obtain the thinner pigment particle of particle diameter by the sulfuric acid solution (D) to 100 Quality Mgmt Dept, and it is also good to make efficient, is therefore preferred.As the mixed proportion between sulfuric acid solution (D) and water (C), with respect to sulfuric acid solution (D) 100 Quality Mgmt Dept, preferred water (C) is 500~1500, is more preferably 700~1200.
Because the liquid temperature by the fluid-mixing that will obtain in the first operation maintains the temperature of the solution state of keeping pigment and maintains below 50 ℃, be easy to obtain less pigment particle of particle diameter, be therefore preferred.Being more preferably liquid temperature is 5 ℃~40 ℃, more preferably 10 ℃~30 ℃.
The temperature of the water (C) that uses due to the first operation is 1 ℃~45 ℃, therefore is easy to obtain liquid temperature and is the fluid-mixing below 50 ℃, is therefore preferred.
Utilize the second operation to carry out cooling to the fluid-mixing that obtains in the first operation.Be adjusted into below 30 ℃ by the temperature with fluid-mixing, and be adjusted into the temperature of keeping solution state when cooling carrying out, can obtain less pigment particle of particle diameter.When the temperature with fluid-mixing is made as below 30 ℃, with in the first operation, moment that obtain to separate out the fluid-mixing that pigment is arranged as Fixed Initial Point, preferably 30 seconds with interior carry out cooling.
The first operation is to carry out in the mixing section of micro-mixer of the present invention, and afterwards, because fluid-mixing is discharged from mixing section, therefore the second operation is carried out outside micro-mixer of the present invention.Carry out the second operation and for example both can be undertaken by batch (-type), also can use the reactors such as pipe reactor cooling continuously.
After the second operation finishes, obtain to have pigment particle to be scattered in dispersion in solution.Both can with this dispersion as end article, also can utilize various means to reclaim particulate, with its dry colour as drying.
In the situation that will utilize pigment particle that manufacture method of the present invention obtains as colouring agent, both can directly use pigment particle that obtains, re-use after also can utilizing surfactant, resin, rosin, pigment derivative etc. to process.
Adopt above-mentioned embodiment, micro-mixer of the present invention can obtain effect as described below.
(1) in the above-described embodiment, micro-mixer 1 has mixing section and be laminated with the laminated section that the second plate forms on the first plate with first small tubulose stream, and, the small tubulose stream of this inlet portion of at least one in the first plate and the second plate is a stream, and being the fluid cross-section that liquid-tight shape ground circulates long-pending in the small tubulose stream of the export department of this plate is to amass little sectional area than be the fluid cross-section that liquid-tight shape ground circulates in a small tubulose stream of inlet portion.By being made as such structure, can improve the mixing efficiency of first fluid and second fluid, even each high viscosity fluid or the anisotropic viscosity fluid that viscosity is different to each other, also can in the situation that do not cause low viscosity fluid intermittently to form stable circulation, can mix efficiently.
Embodiment
Below, utilize embodiment to narrate in further detail the present invention.In example, as long as no particularly pointing out, % is weight basis.
The reaction unit that embodiment 1 uses
Used reaction unit shown in Figure 13 in embodiment 1.In this device, the micro-mixer that uses is micro-mixer shown in Figure 1, and this micro-mixer 1 has laminated section shown in Figure 11.
Micro-mixer 1 is alternately laminated as illustrated in fig. 11 first plate 5, second plate 7 and two temperature control panels 12, this first plate 5 utilizes dry ecthing to be processed to form the first small tubulose stream, this second plate 7 utilizes identical etching and processing to be formed with the second small tubulose stream, and then utilizes two cover plates to clip this duplexer.The material of plate is SUS304.For thickness of slab, plate 5, plate 7 are 0.4mm.Temperature control panel 12 is 1.0mm.The sectional dimension of the small tubulose stream of the first plate 5 is width 0.4mm * degree of depth 0.2mm * length 40mm, and small tubulose stream number is 10.The sectional dimension of the large-diameter portion 8a of the small tubulose stream of the second plate 7 is width 1.2mm * degree of depth 0.2mm * length 20mm.The minor diameter part 8b of tubule shape stream is width 0.4mm * degree of depth 0.2mm * length 2mm, and small tubulose stream number is 10.The sectional dimension of temperature control panel 12 is width 1.2 * degree of depth 0.5 * length 36mm.The area of mixing section is 100mm 2, volume is 300mm 3
In embodiment 1, by utilizing reaction unit synthesis of carbamates acrylate shown in Figure 13, estimated the mixing efficiency of first fluid and second fluid.In Figure 13, the flow export of putting into the container 61 of first fluid is connected by the pipe arrangement that passes through for first fluid with the inflow entrance of plunger displacement pump 63, in addition, the inflow entrance of flow export and plunger displacement pump 64 of putting into the container 62 of second fluid is connected by the pipe arrangement that passes through for second fluid.Be extended with from the flow export of plunger displacement pump 63 and the flow export of plunger displacement pump 64 pipe arrangement that also supplies first fluid or second fluid to pass through by plunger displacement pump 63 or plunger displacement pump 64 respectively, these pipe arrangements are connected with the inflow entrance of micro-mixer 1.
Utilize this micro-mixer 1 to mix first fluid and second fluid, form fluid-mixing.Fluid-mixing distributes with microreactor 65 or 66 to the chemical reaction that is connected side by side by connector 67 by the pipe arrangement that is connected with micro-mixer 1 or 2.Utilize the fluid-mixing that micro-mixer 1 mixes to be respectively allocated to chemical reaction microreactor 65 or 66 corresponding to the time of making fluid-mixing.Mixed solution after distribution reacts in microreactor, and the reactant that obtains is discharged to receiving vessel 68 or 69 by the pipe arrangement that is connected with flow export.
Chemical reaction is microreactor shown in Figure 14 with microreactor 65 or 66, and the laminated section that reacts has structure shown in Figure 15.In Figure 14, α is the fluid-mixing of first fluid and second fluid.β is the reactant of fluid-mixing.γ is the heat exchange medium.
Chemical reaction has two disposable plates and three temperature control panels with microreactor 65 or 66 is alternately laminated, and this disposable plates utilizes dry ecthing to be processed to form five reaction streams 4, and this temperature control panel utilizes identical etching and processing to be formed with five temperature adjustment streams 6.Disposable plates 2 is SUS304 with the material of temperature control panel 3, and thickness of slab is 1mm.The sectional dimension of reaction stream 4 and temperature adjustment stream 6 is width 1.2mm * degree of depth 0.5mm.The length of reaction stream 4 is 40mm.
The device that embodiment 2 uses
The device that embodiment 2 uses is the identical device of device that uses with embodiment 1 except using micro-mixer 2 replacement micro-mixers 1.By coming the synthesizing amino acrylate with this device, estimated the mixing efficiency of first fluid and second fluid.
Micro-mixer 2 has laminated section shown in Figure 16.Micro-mixer 2 is alternately laminated as shown in Figure 14 first plate 5, second plate 7 and two temperature control panels 12, this first plate 5 utilizes dry ecthing to be processed to form the first small tubulose stream, this second plate 7 utilizes etching and processing to be formed with the second small tubulose stream equally, and then this duplexer is clamped by two cover plates.The material of plate is SUS304.For thickness of slab, plate 5, plate 7 are 0.4mm.Temperature control panel 12 is 1.0mm.The area of mixing section is 100mm 2, volume is 300mm 3
For the first small tubulose stream 6, its large-diameter portion 6f is made as width 1.2mm * degree of depth 0.2mm * length 38mm, its minor diameter part 6g is made as width 0.4mm * degree of depth 0.2mm * length 2mm.Small tubulose stream number on the first plate 5 is 10.
The sectional dimension of the large-diameter portion 8a of the small tubulose stream of the second plate 7 is width 1.2mm * degree of depth 0.2mm * length 20mm.The minor diameter part 8b of tubule shape stream is width 0.4mm * degree of depth 0.2mm * length 2mm, and small tubulose stream number is 10.The sectional dimension of the stream of temperature control panel 12 is width 1.2 * degree of depth 0.5 * length (L1) 36mm.
The device that embodiment 3 uses
In embodiment 3, used the device that is connected with the container 61 of putting into first fluid, the container 62 of putting into second fluid, plunger displacement pump and micro-mixer 3.Specifically, the flow export of putting into the container 61 of first fluid is connected by means of the pipe arrangement that passes through for first fluid with the inflow entrance of plunger displacement pump 63, in addition, the inflow entrance of flow export and plunger displacement pump 64 of putting into the container 62 of second fluid is connected by means of the pipe arrangement that passes through for second fluid.Be extended with respectively from the flow export of plunger displacement pump 63 and the flow export of plunger displacement pump 64 pipe arrangement that also supplies first fluid or second fluid to pass through by plunger displacement pump 63 or plunger displacement pump 64, above-mentioned pipe arrangement is connected with the inflow entrance of micro-mixer 3.
Utilize this micro-mixer 3 to mix first fluid and second fluid, be formed with fluid-mixing.Fluid-mixing is discharged to receiving vessel by the pipe arrangement that is connected with micro-mixer 3.
Micro-mixer 3 has the structure that has omitted the temperature control panel 12 in Figure 11.Specifically, micro-mixer 3 is laminated with first plate 5 and second plate 7, and this first plate 5 utilizes dry ecthing to be processed to form the first small tubulose stream, and this second plate 7 utilizes etching and processing to be formed with the second small tubulose stream equally, and then this duplexer is clamped by two cover plates.The material of plate is SUS304.For thickness of slab, plate 5, plate 7 are 0.4mm.The sectional dimension of the small tubulose stream of the first plate 5 is width 0.4mm * degree of depth 0.2mm * length 40mm, and small tubulose stream number is one.The sectional dimension of the large-diameter portion 8a of the small tubulose stream of the second plate 7 is width 1.2mm * degree of depth 0.2mm * length 20mm.The minor diameter part 8b of tubule shape stream is width 0.4mm * degree of depth 0.2mm * length 2mm, and small tubulose stream number is one.
The device that embodiment 4 uses
In embodiment 4, used reaction unit shown in Figure 17.In this device, the micro-mixer 1 that the micro-mixer that uses uses as embodiment 1.
As shown in figure 17, connect container, micro-mixer, heat exchanger and the recovery put into respectively sulfuric acid solution, water contain pigment particle that obtains to some extent the container of dispersion, with it as manufacturing installation.Heat exchanger 69 is microreactor shown in Figure 14, and the laminated section that reacts has structure shown in Figure 15.Heat exchanger 69 is alternately laminated has five disposable plates and seven temperature control panels, this disposable plates to utilize dry ecthing to be processed to form five reaction streams 4, and this temperature control panel utilizes etching and processing to be formed with five temperature adjustment streams 6 equally.Disposable plates 2 is SUS304 with the material of temperature control panel 3, and thickness of slab is 1mm.Reaction stream 4 is width 1.2mm * degree of depth 0.5mm with the sectional dimension of temperature adjustment stream 6.The length of reaction stream 4 is 40mm.
Embodiment 1
To used as the 1st fluid, viscosity is adjusted into the isocyanate compound of 2mPas and carries out the synthetic of amino acrylates as second fluid, polyfunctional acrylic ester that viscosity is adjusted into 300mPas.Adjustment refers to by carrying thermal mediums to temperature control panel 12, and the temperature of each fluid is made as 60 ℃.
Utilize plunger displacement pump 63 and 64 to make above-claimed cpd with flow velocity 100g/min circulation, and by making it obtain fluid-mixing in the interior circulation of micro-mixer 1.The fluid-mixing that obtains is divided into initial stage, two stages of later stage, and the operation connector is supplied to microreactor 65 and 66 with the fluid-mixing that obtains respectively.The fluid-mixing that obtains is reacted with 160 ℃, the conditions of 50 seconds holdup times in each microreactor.To use microreactor 65 and 66 amino acrylates that obtain to be designated as briefly respectively amino acrylates (1-1), amino acrylates (1-2).Result according to gel permeation chromatography (GPC) analysis, amino acrylates Area Ratio (%) in amino acrylates (1-1) is respectively 95 (%), 1.3 (%) with the Area Ratio (%) of surplus acrylate, amino acrylates Area Ratio (%) in amino acrylates (1-2) is respectively 95 (%), 1.3 (%) with the Area Ratio (%) of surplus acrylate, is identical value.Thus, think and utilize micro-mixer 1 to mix well.
Embodiment 2
To used as first fluid, viscosity is adjusted into the isocyanate compound of 100mPas and carries out the synthetic of amino acrylates as second fluid, polyfunctional acrylic ester that viscosity is adjusted into 300mPas.Adjustment refers to temperature control panel 12 and carries thermal mediums, and the temperature of each fluid is made as 60 ℃.
Utilize plunger displacement pump 63 and 64 to make above-claimed cpd with flow velocity 100g/min circulation, and by making it obtain fluid-mixing in the interior circulation of micro-mixer 1.The fluid-mixing that obtains is divided into initial stage, two stages of later stage, and the operation connector is supplied to microreactor 65 and 66 with the fluid-mixing that obtains respectively.The fluid-mixing that obtains is reacted with 160 ℃, the conditions of 50 seconds holdup times in each microreactor.To use microreactor 65 and 66 amino acrylates that obtain to be designated as briefly respectively amino acrylates (1-1), amino acrylates (1-2).Result according to gel permeation chromatography (GPC) analysis, amino acrylates Area Ratio (%) in amino acrylates (1-1) is respectively 95.5 (%), 1.3 (%) with the Area Ratio (%) of surplus acrylate, amino acrylates Area Ratio (%) in amino acrylates (1-2) is respectively 95.5 (%), 1.3 (%) with the Area Ratio (%) of surplus acrylate, is identical value.Thus, think and to utilize micro-mixer 2 to mix well.
In embodiment 1, the flow velocity of the first fluid of the export department of the small tubulose stream in the mixing section of micro-mixer of the present invention is 0.42m/s, and the speed of second fluid is 1.66m/s.
Embodiment 3
Utilize plunger displacement pump, the water of viscosity 1mPas and maltose condition with flow velocity 10g/min in having the device of micro-mixer of viscosity 30mPas are circulated.Its result has been confirmed and can have been mixed in pulseless mode.
Embodiment 4
As the pigment with anthraquinone structure, mix with the ratio of the concentrated sulfuric acid of 98 quality % with respect to the C.I paratonere 177 of 1g, obtained sulfuric acid solution (normal temperature viscosity the 27mPas) (containing ratio of the pigment in sulfuric acid solution: 12.5 quality %).Liquid temperature during dissolving pigment is 37 ℃, and mixing time is 2 hours.Sulfuric acid solution 100g is put into the container 62 of device shown in Figure 17, in addition, water 1500g is put into container 64.
Use plunger displacement pump 65 and 66, with the ratio of weight ratio 1:10, and form with flow the mode that 88g/ divides the water in the sulfuric acid solution in container 62 and container 64 is supplied to micro-mixer 67, utilize the micro-mixer acquisition to contain the fluid-mixing of pigment particle.The liquid temperature (T1) of the fluid-mixing of this moment is 40 ℃.Then, mixed solution is carried to heat exchanger, having obtained liquid temperature (T2) is the dispersion of pigment particle of 25 ℃.As Fixed Initial Point, (T1) is adjusted into the time that temperature (T2) spends is 15 seconds with moment of obtaining mixed solution (A).In addition, water circulates in the small tubulose stream that the first plate has, and sulfuric acid solution circulates in the small tubulose stream that the first plate has.
The mean particle diameter of pigment particle in the dispersion 1 of pigment particle that obtains (the SAXS particle diameter that is obtained by the small-angle scattering method) is 10.1nm.
Comparative example 1
Except using Y-shaped micro-mixer replacement micro-mixer 3, carried out the combined experiments of anisotropic viscosity fluid in the mode identical with embodiment 3.Being arranged at stream this Y-shaped micro-mixer, confession the 1st Fluid Flow in A is width 0.4mm * degree of depth 0.2mm * length 15mm.Be identical width 0.4mm * degree of depth 0.2mm * length 15mm for the stream of the 2nd Fluid Flow in A.In addition, the stream that flows for mixed liquor is width 0.8mm * degree of depth 0.2 * length 15mm.Because the material of the plate that has formed stream is identical with micro-mixer 1, so the thickness of stream wall is identical with micro-mixer 1.
The result of experiment can confirm, and finds to have intermittently circulation in as the water of low viscosity fluid, and stable circulation is difficulty comparatively.That is, because the Y-shaped blender is by each stream being intersected make the design at each fluid interflow, therefore when mobile when the different two kinds of fluids of viscosity are arranged in each stream, want to make low viscosity fluid identical with the crushing of high viscosity fluid.In this experiment, the cross section of interflow section is 0.8mm * degree of depth 0.2mm=0.16mm 2, with respect to the cross section 0.16 * 30/31=0.155mm that flows for high viscosity fluid 2, the cross section of low viscosity fluid side is 0.16 * 1/31=0.005mm 2, because the cross section of flowing for low viscosity fluid is minimum, therefore can infer to produce intermittent entry.
Comparative example 2
Except the micro-mixer that embodiment was used with the flat 9-512742 of Japanese Unexamined Patent Application Publication replaces micro-mixer 1, and, the mode that forms 12.5g/min with the flow in when circulation utilizes plunger displacement pump to make respectively outside flow passes to, and has obtained in the same manner amino acrylates (2 '-1), amino acrylates (2 '-2) with embodiment 1.The sectional dimension of the first plate that the micro-mixer that the embodiment of the flat 9-512742 of Japanese Unexamined Patent Application Publication uses has, the small tubulose stream of the 2nd plate is width 0.4mm * degree of depth 0.2mm * length 40mm, and small tubulose stream number is 10.The laminates number is each.
Amino acrylates Area Ratio (%) in the amino acrylates that obtains (2 '-1) is 92 (%), the Area Ratio of surplus acrylate (%) is 2.7 (%), amino acrylates Area Ratio (%) in the amino acrylates that obtains (2 '-2) is 77 (%), the Area Ratio of surplus acrylate (%) is 18.8 (%), and Area Ratio is different.According to this result, draw the following conclusions: generating has the different amino acrylates of physical property values, does not mix uniformly.In addition, though want to circulate with 100g/min, be more than high viscosity 10MPa but viscosity is adjusted into the polyfunctional acrylic ester crushing of 300mPas, be difficult to circulate, can't obtain amino acrylates.
Description of reference numerals
The housing of C, micro-mixer 1; The left end of C1, housing C; The bottom right-hand member of C2, housing C; The bottom left end of C3, housing C; The upper end of C4, housing C; F1, first fluid; F2, second fluid; The fluid-mixing of F3, first fluid and second fluid; H1, thermal medium; S1, the reservoir of temporarily accumulating the 1st fluid (F1); S2, the reservoir of temporarily accumulating the 2nd fluid (F2); S3, mixing section; 1A, the 1st fluid supply unit; 1B, be formed at the peristome of the left part of housing C; 1C, the connector that is connected with peristome 2B; 2A, the 2nd fluid supply unit; 2B, be formed at the peristome of the bottom right-hand member of housing C; 2C, the connector that is connected with peristome 2B; 3A, the thermal medium supply unit that thermal medium H1 is supplied with in the housing C; 3B, be formed at the peristome of the bottom left end of housing C; 3C, the connector that is connected with peristome 3B; 4A, thermal medium efferent; 4B, be formed at the peristome of the upper right end of housing C; 4C, the connector that is connected with peristome 4B; 5, the first plate; 5A, the efferent that is consisted of by peristome 5B and connector 5C; 5B, be formed at the peristome of the right part of housing C; 5C, the connector that is connected with peristome 5B; 6, the first small tubulose stream; 6A, the first small tubulose stream forming portion; The upper surface of 6a, the first small tubulose stream forming portion 6A; The left-hand end of 6b, the first small tubulose stream forming portion 6A; The right-hand end of 6c, the first small tubulose stream forming portion 6A; The entrance of 6d, the first small tubulose stream 6; The outlet of 6e, the first small tubulose stream 6; 7, the second plate; 7A, the second small tubulose stream forming portion; The upper surface of 7a, the second small tubulose stream forming portion 7A; The lower side of 7b, the second small tubulose stream forming portion 7A; 7c, be positioned at the end on width from the lower side 7b of the second small tubulose stream forming portion 7A; The right-hand end of 7d, the second small tubulose stream forming portion 7A; 8, the second small tubulose stream; The entrance of 8a, the second small tubulose stream 8; The outlet of 8b, the first small tubulose stream 6; 9, the larger large-diameter portion of stream diameter in the second small tubulose stream 8; 10, the less minor diameter part of stream diameter in the second small tubulose stream 8; 11, the tapering in the second small tubulose stream 8; 12, temperature control panel; The face of 12a, temperature control panel 12; 13, be arranged at the temperature adjustment stream of the section grooves shape on the face 12a of temperature control panel 12; 13a, be arranged with the primary flow path of many along the length direction of temperature control panel 12; 13b, the supply side stream that is communicated with primary flow path 13a; 13c, the discharge effluent road that is communicated with primary flow path 13a; 61, put into the container of first fluid; 62, put into the container of second fluid; 63, plunger displacement pump; 64, plunger displacement pump; 65, pipe reactor; 66, pipe reactor; 67, connector; 68, receiving vessel; 69, receiving vessel; 70, the sulfuric acid solution of pigment; 71, the 1st container; 72, water; 73, the 2nd container; 74, plunger displacement pump; 75, plunger displacement pump; 76, micro-mixer; 77, register; 78, the cooling heat exchanger of using; 79, purge valve; 80, reaction unit; 81, receiving vessel; 110, duplexer.

Claims (8)

1. micro-mixer, it is characterized in that, this micro-mixer has laminated section and mixing section, this laminated section forms by on the first plate, being laminated with the second plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid, this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid, this mixing section is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, and mixing first fluid and second fluid
The inlet portion of the small tubulose stream that is communicated with the fluid feed path of at least one in the first plate and the second plate is a stream, and the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of this at least one the export department that is communicated with mixing section is little.
2. micro-mixer according to claim 1, is characterized in that,
The sectional area of the small tubulose stream of the inlet portion of the small tubulose stream that the sectional area ratio of the small tubulose stream of the export department that is communicated with mixing section of above-mentioned the first plate is communicated with the fluid feed path is little,
The inlet portion of the small tubulose stream that is communicated with the fluid feed path of the second plate is a stream, and the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of the export department that is communicated with mixing section of the second plate is little.
3. micro-mixer according to claim 1, is characterized in that,
The sectional area of a small tubulose stream of above-mentioned inlet portion is 0.01mm 2~40mm 2, the sectional area of the small tubulose stream of export department is 0.01mm 2~10mm 2
4. micro-mixer according to claim 1, is characterized in that,
Also be laminated with temperature control panel at above-mentioned laminated section, this temperature control panel has the heat transferring medium stream that makes the heat transferring medium circulation.
5. micro-mixer according to claim 1, is characterized in that,
10 times~200 times of the summation of the sectional area of the sectional area of section and the outlet that the area cross section that outlet outlet the first small tubulose stream and the second small tubulose stream is communicated with is the first small tubulose stream of above-mentioned mixing and the outlet of the second small tubulose stream, the export department of the export department of the above-mentioned first small tubulose stream and the second small tubulose stream be 2mm~100mm for the distance between the export department of the section of mixing of the mixture circulation of first fluid and second fluid.
6. the manufacture method of a mixed liquor, is characterized in that,
This manufacture method is used following micro-mixer, and making ratio of viscosities is that 10~3000 first fluid and second fluid circulate in the first small tubulose stream and the second small tubulose stream respectively, contains the fluid-mixing of first fluid and second fluid in the acquisition of mixing section,
above-mentioned micro-mixer has laminated section and mixing section, this laminated section forms by be laminated with the second plate on the first plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid, this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid, this mixing section is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, and mixing first fluid and second fluid, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of at least one in the first plate and the second plate is a stream, and, the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of this at least one the export department that is communicated with mixing section is little.
7. the manufacture method of a polyurethane (methyl) acrylate, is characterized in that,
use the micro-mixer of following feature: this micro-mixer has laminated section and mixing section, this laminated section forms by be laminated with the second plate on the first plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid, this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid, this mixing section is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, and mixing first fluid and second fluid, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of at least one in the first plate and the second plate is a stream, and, the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of this at least one the export department that is communicated with mixing section is little,
The manufacture method of above-mentioned polyurethane (methyl) acrylate comprises:
The first operation, make in any one in the above-mentioned first small tubulose stream or the second small tubulose stream of compound (A) with NCO and circulate, (methyl) acrylate (B) with hydroxyl is circulated in another small tubulose stream, obtain to contain compound (A) and compound (B) at interior fluid-mixing in mixing section; And
The second operation makes the compound (A) in this fluid-mixing react with compound (B).
8. the manufacture method with pigment particle of anthraquinone structure, is characterized in that,
use the micro-mixer of following feature: this micro-mixer has laminated section and mixing section, this laminated section forms by be laminated with the second plate on the first plate, this first plate has the first small tubulose stream that is communicated with the fluid feed path that circulates for first fluid, this second plate has the second small tubulose stream that is communicated with and supplies the second fluid circulation with the fluid feed path that circulates for second fluid, this mixing section is communicated with the outlet of the first small tubulose stream and the outlet of the second small tubulose stream, and mixing first fluid and second fluid, the inlet portion of the small tubulose stream that is communicated with the fluid feed path of at least one in the first plate and the second plate is a stream, and, the sectional area of the small tubulose stream of the sectional area ratio inlet portion of the small tubulose stream of this at least one the export department that is communicated with mixing section is little,
Above-mentioned manufacture method with pigment particle of anthraquinone structure comprises:
The first operation, make in any one in the above-mentioned first small tubulose stream and the second small tubulose stream of water (C) and circulate, the sulfuric acid solution (D) of the pigment with anthraquinone structure is circulated in another small tubulose stream, at mixing section's mixing water (C) and sulfuric acid solution (D), obtain to have separated out the fluid-mixing of the pigment with anthraquinone structure; And
The second operation is carried out cooling to the fluid-mixing of having separated out this pigment.
CN2011800474568A 2010-09-30 2011-09-27 Micromixer Pending CN103140279A (en)

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JP6044199B2 (en) * 2012-09-05 2016-12-14 Dic株式会社 Method for producing polymer
JP2017148796A (en) * 2016-02-24 2017-08-31 東芝機械株式会社 Micromixer, micromixer element, and manufacturing method of the same
JP6808259B1 (en) * 2020-06-12 2021-01-06 合同会社アプテックス Laminated Venturi nozzle, its manufacturing method, and micro-bubble liquid generator
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